CN101319282B - Method for manufacturing high-density vanadium-nitrogen alloy - Google Patents
Method for manufacturing high-density vanadium-nitrogen alloy Download PDFInfo
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- CN101319282B CN101319282B CN2008100223729A CN200810022372A CN101319282B CN 101319282 B CN101319282 B CN 101319282B CN 2008100223729 A CN2008100223729 A CN 2008100223729A CN 200810022372 A CN200810022372 A CN 200810022372A CN 101319282 B CN101319282 B CN 101319282B
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- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001199 N alloy Inorganic materials 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000003763 carbonization Methods 0.000 claims abstract description 10
- 230000005389 magnetism Effects 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- 229910045601 alloy Inorganic materials 0.000 claims description 14
- 239000000956 alloy Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 abstract description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000831 Steel Inorganic materials 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 239000010959 steel Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 3
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract 1
- 239000007767 bonding agent Substances 0.000 abstract 1
- 238000005121 nitriding Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract 1
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 239000000843 powder Substances 0.000 description 5
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 241000723346 Cinnamomum camphora Species 0.000 description 4
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 4
- 229960000846 camphor Drugs 0.000 description 4
- 229930008380 camphor Natural products 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910000592 Ferroniobium Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 229940087654 iron carbonyl Drugs 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for producing vanadium-nitrogen alloy. In the method, powdered vanadium oxide or ammonium metavanadate, carbon powder, bonding agents and density increasing agents are evenly mixed and are subjected to briquetting and forming; the mixture is continuously added in an external-heat type rotary kiln under the atmosphere of nitrogen gas and preheated up to the temperature of below 1,000 DEG C under the protection of the nitrogen gas, and at a discharge port, preheated massive products which are cooled down to the room temperature under the protection of nitrogen gas are collected; and the massive products are put in an improved soft magnetism nitrogen atmosphere kiln and heated up to the temperature of between 1,000 and 1,500 DEG C so as to make materials carryout the carbonization reaction and the nitriding reaction, and the vanadium-nitrogen alloy products are obtained after discharge. In the vanadium-nitrogen alloy obtained, the V content is between 78 and 83 percent, the N content is between16 and 21 percent, the C content is less than or equal to 6 percent max, the contents of silicon, phosphor and aluminum are less than 0.01 percent, and the apparent density is more than 4.4g/cm<3>. The apparent density can be adjusted according to the requirements of a customer, and the maximum apparent density is 5.0 g/cm<3>. The method is characterized in that under the condition of not changing prior production processes, the apparent density of the vanadium-nitrogen alloy is improved by adding the density increasing agents, and the adsorption rate ofmolten steel in the vanadium-nitrogen alloy is more than 98 percent.
Description
Technical field
The present invention is a kind of method of high density production VN alloy, belongs to field of new.
Background technology
Nineteen twenty-five, the charcoal that utilizes pine tree to burn till, Friederich and Sittig (E.Friederich and L.Sittig, Z.Anorg.Allg.Chem., 1925,144,169) are with V
2O
3Be raw material, prepared vanadium nitride at 1200 ℃.
1975, reduce Vanadium Pentoxide in FLAKES with ammonia, people such as Guidotti (R.A.Guidotti, G.B.Atkinsonand D.G.Kesterke, Report of Investigation No.8079, US Bureau of Mines, Washington DC, 1975) also obtain vanadium nitride.
Nineteen ninety-five, adopt methane under 1180 ℃, Rajat and S.T.Oyama (Journal of Solid StateChemistry, 1995,120, the 320-326) method of the synthetic vanadium carbide of reduction Vanadium Pentoxide in FLAKES.
2000, adopt Vanadium Pentoxide in FLAKES, at high temperature 1200-1800 ° in medium-frequency induction furnace reduction with carbon method, Prabhat Kumar Tripathy[Journal of Materials Chemistry, 2001,11,691-695)] prepared vanadium nitride.
2003, people [Chemistry Letters Vol.32, No.3 (2003)] such as Xiaogang Yang reported nanocrystalline vanadium nitride achievement in research.
In above-mentioned research, or do not mention apparent density, or can only be used as the additive of powder metallurgy for the powder sample.
The Nitrovan12 of VANITEC company and Nitrovan16 product apparent density are more than or equal to 3.0g/cm
3
Patent application 01139886.8, its apparent density is greater than 3.0 g/cm
3, maximum apparent density is not more than 4.3g/cm among the embodiment
3
Summary of the invention
The production method that the purpose of this invention is to provide a kind of high-density vanadium-nitrogen alloy can increase the apparent density of block vanadium-nitrogen alloy product, and VN alloy is sunk in the molten steel effectively, improves the specific absorption of molten steel to VN alloy.
Technical solution of the present invention:
The production method of VN alloy is characterized in that:
(1), raw material weight proportioning:
Described density dose is selected from: the solution or the colloid of irony, niobium matter pulvis, comprise one or more of following composition: iron powder, nanometer iron powder, iron carbonyl, Z 250, iron oxide black, ferric oxide, contain iron oxide red, the smart iron ore of high product, rhombohedral iron ore, iron scale, ironic hydroxide and ferrous hydroxide; The niobium powder, Niobium Pentxoxide; The ferrocolumbium powder; Described carbonaceous pulvis is selected from gac; Described binding agent is selected PVP solution or camphor solution for use;
(2), preparation technology:
Earlier with pulverous barium oxide or ammonium meta-vanadate or the mixture of the two, carbonaceous pulvis and binder solution; add density dose powder; mix back briquetting, moulding; in external-heating rotary kiln, under the nitrogen protection after 800-1000 ℃ of pre-burning, under nitrogen protection atmosphere, cool off, subsequently in nitrogen atmosphere soft magnetism stove; be heated to 1000-1500 ℃ of temperature; time is 3-10 hour, and material generation carbonization and nitrogenizing reaction promptly obtain highdensity vanadium-nitrogen alloy product after cooling is come out of the stove.
Described PVP strength of solution is 1-5%, and camphor solution is the acetone soln that contains camphor 3-5%.Described density dose feeds intake with solution or powder form.
The production method of described VN alloy is characterized in that:
(1), described raw material weight proportioning:
(2), preparation technology:
Earlier with pulverous barium oxide or ammonium meta-vanadate or the mixture of the two, carbonaceous pulvis and binder solution; add density dose powder; mix back briquetting, moulding; after 800-900 ℃ of pre-burning under the nitrogen protection in external-heating rotary kiln; in nitrogen atmosphere soft magnetism stove, be heated to 1200-1450 ℃ of temperature, the time is 3-10 hour; material generation carbonization and nitrogenizing reaction promptly obtain highdensity vanadium-nitrogen alloy product after cooling is come out of the stove.
The production method of described VN alloy is characterized in that:
(1), described raw material weight proportioning:
(2), preparation technology
With material component back briquetting, the moulding that stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 800-900 ℃ in advance; collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port, push then in the nitrogen atmosphere soft magnetism stove, be heated to 1260-1400 ℃ of temperature; time 4-6 hour; in dynamic successive processes, material generation carbonization and nitrogenizing reaction promptly obtain highdensity vanadium-nitrogen alloy product after cooling is come out of the stove.
The production method of described VN alloy is characterized in that:
(1), described raw material weight proportioning:
(2), preparation technology
With material component back briquetting, the moulding that stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 830-880 ℃ in advance; collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port; push then in the nitrogen atmosphere soft magnetism stove, be heated to 1 370-1450 ℃ temperature, time 3-5 hour; in dynamic successive processes, material generation carbonization and nitrogenizing reaction.
The production method of described VN alloy is characterized in that:
(1), described raw material weight proportioning:
(2), preparation technology
With material component back briquetting, the moulding that stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 900-950 ℃ in advance; collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port; push then in the nitrogen atmosphere soft magnetism stove, be heated to 1430 ℃ of temperature, time 3-4 hour; in dynamic successive processes, material generation carbonization and nitrogenizing reaction.
Compared with the prior art the present invention has following advantage:
1, do not need the newly added equipment investment, change original production technique,, just can by adding the density dose
To increase the density of VN alloy, improve the specific absorption of molten steel to VN alloy.
2, substituted and need to improve the method for apparent density by a small margin before adding by long-time insulation.Therefore,
The production efficiency that present method has obviously improved has been saved the energy.
3, constant product quality, the apparent density height, and can adjust according to client's demand.
Embodiment
Embodiment 1
The gac of the Vanadium Pentoxide in FLAKES of 603kg (containing vanadium 55.2%) and 182kg; containing PVP with 60kg is 1% the aqueous solution; the colloidal solution that adds 6kg nanometer iron powder and iron carbonyl; back briquetting, moulding stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 800 ℃ in advance, collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port.Push then in the improved soft magnetism nitrogen atmosphere stove, be heated to 1260 ℃ of temperature.In dynamic successive processes, material generation carbonization and nitrogenizing reaction.5 hours residence time promptly obtained vanadium-nitrogen alloy product after coming out of the stove altogether in the high-temperature zone.The VN alloy that the present invention makes: V:78.2%, N:16.7%, C:3.8%, silicon, phosphorus and aluminium less than: 0.10%, its apparent density is greater than 4.8g/cm
3
Embodiment 2
The ammonium meta-vanadate of the vanadiumcontent 42.9% of 823kg and the gac of 276kg; contain the aqueous solution of PVP1% with 47kg; briquetting, moulding after adding 7kg Z 250, ferric oxide and ferrocolumbium stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 830 ℃ in advance, collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port.Push then in the improved soft magnetism nitrogen atmosphere stove, be heated to 1370 ℃ of temperature.In dynamic successive processes, material generation carbonization and nitrogenizing reaction.5 hours residence time promptly obtained vanadium-nitrogen alloy product after coming out of the stove altogether in the high-temperature zone.The VN alloy that the present invention makes: V:78.5%, N:17.9%, C:2.3%, silicon, phosphorus and aluminium less than: 0.10%, its apparent density is greater than 4.4g/cm
3
Embodiment 3
The gac of the Vanadium Pentoxide in FLAKES of the vanadiumcontent 55.6% of 367kg and 423kg vanadiumcontent 42.9% ammonium meta-vanadate and 259kg; containing PVP with 50kg is the acetone soln that 1% the aqueous solution and 5kg contain camphor 3%; add 8kg Z 250, ferric hydroxide colloid and niobium powder; back briquetting, moulding stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 900 ℃ in advance, collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port.Push then in the improved soft magnetism nitrogen atmosphere stove, be heated to 1430 ℃ of temperature.In dynamic successive processes, material generation carbonization and nitrogenizing reaction.3 hours residence time promptly obtained vanadium-nitrogen alloy product after coming out of the stove altogether in the high-temperature zone.The VN alloy that the present invention makes: V:79.5%, N:18.7%, C:0.3%, silicon, phosphorus and aluminium less than: 0.10%, its apparent density is greater than 5.0g/cm
3
Claims (1)
1. the production method of VN alloy is characterized in that:
(1), described raw material weight proportioning:
(2), preparation technology
With material component back briquetting, the moulding that stir; under nitrogen atmosphere, add external-heating rotary kiln continuously; under nitrogen protection, burn 830-880 ℃ in advance; collect the bulk product that under nitrogen protection, is cooled to the pre-burning of room temperature at discharge port, push then in the nitrogen atmosphere soft magnetism stove, be heated to 1370-1450 ℃ of temperature; time 3-5 hour; in dynamic successive processes, material generation carbonization and nitrogenizing reaction promptly obtain highdensity vanadium-nitrogen alloy product after cooling is come out of the stove.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100223729A CN101319282B (en) | 2008-06-28 | 2008-06-28 | Method for manufacturing high-density vanadium-nitrogen alloy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100223729A CN101319282B (en) | 2008-06-28 | 2008-06-28 | Method for manufacturing high-density vanadium-nitrogen alloy |
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| CN101319282A CN101319282A (en) | 2008-12-10 |
| CN101319282B true CN101319282B (en) | 2011-08-17 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011098B (en) * | 2012-11-29 | 2017-05-24 | 湖南省宏元稀有金属材料有限公司 | Production method for increasing content of nitrogen in vanadium-nitrogen alloy |
| CN103305739B (en) * | 2013-07-09 | 2015-10-21 | 高博 | A kind of high nitrogen VN alloy VN18 and production method thereof |
| CN105986140A (en) * | 2015-01-30 | 2016-10-05 | 新疆众豪钒业科技有限公司 | Method and apparatus for producing vanadium nitrogen alloy by using ammonium metavanadate |
| CN105039772B (en) * | 2015-06-30 | 2018-01-19 | 河北钢铁股份有限公司承德分公司 | The method that continuous high-efficient produces high nitrogen content VN alloy |
| CN107699779A (en) * | 2017-08-29 | 2018-02-16 | 湖北华祥合金有限公司 | A kind of VN alloy and its production method |
| CN110184521B (en) * | 2019-06-17 | 2021-04-23 | 承德燕北冶金材料有限公司 | Composite densifier and method for preparing vanadium-nitrogen alloy by adopting same |
| CN113430402B (en) * | 2021-06-07 | 2022-02-01 | 湖南众鑫新材料科技股份有限公司 | Raw material forming method in vanadium-nitrogen alloy production process |
| CN113684363B (en) * | 2021-08-05 | 2022-09-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for producing vanadium-nitrogen alloy with preset sulfur content |
| CN114395708A (en) * | 2021-11-16 | 2022-04-26 | 陕西华银科技股份有限公司 | Key process for preparing vanadium-nitrogen alloy by mixing ammonium metavanadate and vanadium pentoxide |
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